CN102978738A - Method for manufacturing conductive polypropylene fibers - Google Patents
Method for manufacturing conductive polypropylene fibers Download PDFInfo
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- CN102978738A CN102978738A CN2012104913791A CN201210491379A CN102978738A CN 102978738 A CN102978738 A CN 102978738A CN 2012104913791 A CN2012104913791 A CN 2012104913791A CN 201210491379 A CN201210491379 A CN 201210491379A CN 102978738 A CN102978738 A CN 102978738A
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Abstract
The invention discloses a method for manufacturing conductive polypropylene fibers. The method comprises the following steps of: A) uniformly mixing tetrapod-shaped zinc oxide whiskers with conductive potassium titanate whiskers, baking the mixture in a vacuum furnace, cooling, then dispersing by stirring in absolute ethyl alcohol containing sodium hexametahposphate, performing plasma treatment at normal pressure, and performing ultrasonic dispersion, cleaning, filtering and drying in deionized water containing a calcium stearate dispersion liquid to obtain a modified whisker mixture; B) mixing and stirring the modified whisker mixture with antimony doped tin oxide conductive powder, superconducting carbon black, an aluminate coupling agent, polyethylene wax and a PP-g-MAH compatibilizer, adding isotactic polypropylene powder into the mixture, and stirring to obtain a conductive isotactic polypropylene blend; and C) preparing the conductive isotactic polypropylene blend and other compatible polypropylene (PP) or polyethylene (PE) into the conductive polypropylene fibers with the conductive polypropylene as a skin layer through composite spinning.
Description
Technical field
The present invention relates to a kind of manufacture method of conducting polypropylene fiber, comprise ZnOw (ZnO), electric conductivity potassium titanate crystal whisker (PTW), the ATO conducting powder, the manufacture method of the fibers such as superconductive carbon black belongs to the functional fibre manufacturing technology.
Background technology
Polypropylene fibre is also claimed PP fiber or polypropylene fibre, is a kind of fiber with the isotactic polypropylene melt-spinning, and its great advantage is light weight, and its density is 0.91/cm
3, than the light 20-30% of general chemical fibre, be a kind of of proportion minimum in all textile fabrics, its intensity is high, and elongation is large, and initial modulus is higher, excellent spring.The polypropylene fibre ABRASION RESISTANCE is only second to polyamide fiber; Corrosion resistance is good, and is especially fine to inorganic acid, alkaline stability; Not mouldy, without putrefaction is not afraid of and is damaged by worms etc.; But polypropylene fibre does not absorb water, and static is very large, and the normal temperature specific insulation is up to 10
17Ω .cm,, be very limited in application.
Conductive fiber typically refers under standard state (20 ℃, 65% relative humidity), than resistance 10
7The fiber that Ω cm is following.Therefore this fibrid has good electric conductivity and durability, particularly still has good durable electric conductivity under low humidity, in the field such as industrial, civilian very large purposes is arranged.At present, conductive fiber is matrix mainly with common fiber-forming polymer greatly, add the conductive fiber of conductive materials with coating or complex method, make the part of fiber contain conductive materials by composite spinning technology, make like this fiber when having conductive characteristic, have again the processing characteristics of common synthetic fiber excellence concurrently, become the conductive fiber with spinnability.Along with high-tech development, aspect civilian and industry usefulness, the demand of conductive fiber is increasing, and it is higher to require also to get up.
Whisker be the diameter that forms with monocrystalline form growth very little (0.1～10um), atomic arrangement high-sequential, intensity near the theoretical value of perfect crystal, the fibrous material of certain draw ratio (5～1000) is arranged, have high strength, high-modulus, high rigidity, the characteristic such as high temperature resistant, corrosion-resistant; Add a small amount of whisker in the isotactic polypropylene, such as ZnOw, calcium carbonate crystal whisker, potassium titanate crystal whisker etc., just can not only strengthen but also toughness reinforcing, also can improve electric conductivity.
In the whisker of this numerous kinds, four acicular type zinc oxide crystal whisker (ZnO) is given its outstanding electric conductivity with solid four acicular textures of its uniqueness; ZnO itself is the N-shaped semiconductor, and four-feet needle-shaped whisker three-dimensional extension structure when being dispersed in it in matrix, being close to each needle-like position and mutually being overlapped the formation conductive path in addition, electric charge is conducted, thereby give material electric conductivity.Electric conductivity potassium titanate crystal whisker (PTW) is a kind of needle-like staple fibre compound, because its size is tiny, perfect crystalline has the physical and mechanical propertiess such as conduction.
The scientific worker is take common fibroblast high molecular polymer as matrix for many years, develop the macromolecular material conductive fiber to add the conductive materials mode, make like this fiber when having conductive characteristic, have again the processing characteristics of common synthetic fiber excellence concurrently, become the functional fiber with spinnability, but the electric conductivity of polymer matrix conductive fiber, fibre strength all are not so good as the metallic conduction fiber, and the metallic conduction fiber is too hard, lack flexibility, in use be very limited.
Summary of the invention
The object of the invention is to overcome the deficiency that prior art exists,, a kind of have good electric conductivity and durability are provided, particularly under low humidity, still have the manufacture method of good durable conducting polypropylene fiber from natural disposition electric conductivity.
The objective of the invention is to finish by following technical solution, a kind of manufacture method of conducting polypropylene fiber, this manufacture method comprises the steps:
A) getting 12-18 part characterization parameter diameter by mass fraction is 0.2-1um, and length is the four acicular type zinc oxide crystal whisker of 5-15um; 3-8 part characterization parameter diameter is 0.2-0.6um, and length is the electric conductivity potassium titanate crystal whisker of 5-12um; After above-mentioned material mixed, at 300-400 ℃ of vacuum kiln roasting 4-6h; With calgon dispersed with stirring in absolute ethyl alcohol, then atmospheric plasma is processed 10-20min after the cooling; With 60-70 ℃ of loose, the cleaning 25-35min of deionized water for ultrasonic wavelength-division that contains calcium stearate dispersion, get solution upper strata suspension whisker and filter through 100 orders～150 orders, get the modified crystal whiskers mixed liquor, and repetitive operation 3-5 time is until filtering; In the vacuum drying oven oven dry, obtain the modified crystal whiskers mixture after the filtering;
B) get steps A by mass fraction) modified crystal whiskers mixture 6-10 part of obtaining, antimony doped tin oxide conducting powder 3-5 part, superconductive carbon black 7-17 part, aluminate coupling agent 0.2-0.4 part, Tissuemat E 1.7-3.0 part, PP-g-MAH bulking agent 1.2-2.5 part, mixer 250-400 turns/the airtight stirring reaction 45-60min of min under 60-70 ℃ of condition; And then adding isotactic polypropylene powder 100-120 part, 300-400 turns/min stirs 30-45min, obtains conducting electricity the isotactic polypropylene blend;
C) with step B) the conduction isotactic polypropylene blend that obtains at the dynamic vacuum oven drying to moisture content≤35ppm, directly extrude at the parallel dual-screw melting extruder that mixes, having the PP of compatibility or PE to make conduction isotactic polypropylene blend through composite spinning by core-skin mass ratio 20-30 ﹕ 80-70 and other is the polypropylene conductive fiber of cortex.
The preferred technical scheme of the present invention is: described manufacture method, wherein:
Steps A) getting 15 parts of characterization parameter diameters by mass fraction in is 0.2-1um, and length is the four acicular type zinc oxide crystal whisker of 5-15um; 5 parts of characterization parameter diameters are 0.2-0.6um, and length is the electric conductivity potassium titanate crystal whisker of 5-12um; After above-mentioned material mixed, at 350 ℃ of vacuum kiln roasting 4-6h; With calgon dispersed with stirring in absolute ethyl alcohol, atmospheric plasma is processed 10-20min after the cooling; Then with 60-70 ℃ of loose, the cleaning 30min of deionized water for ultrasonic wavelength-division that contains calcium stearate dispersion, get solution upper strata suspension whisker and filter through 120 orders, get the modified crystal whiskers mixed liquor, and repetitive operation 3-5 time is until filtering; In the vacuum drying oven oven dry, obtain the modified crystal whiskers mixture after the filtering;
Step B) in, get steps A by mass fraction) 8 parts in the modified crystal whiskers mixture that obtains, 4 parts of antimony doped tin oxide conducting powder, 10 parts of superconductive carbon blacks, 0.3 part of aluminate coupling agent, 2.0 parts of Tissuemat Es, 2.0 parts of PP-g-MAH bulking agents, mixer 320 turns/the airtight stirring reaction 50min of min under 65 ℃ of conditions; And then add 100 parts in isotactic polypropylene powder, and 350 turn/min stirs 38min, obtain conducting electricity the isotactic polypropylene blend.
The conducting polypropylene fiber that the present invention makes is to add to comprise the ATO conducting powder in polypropylene, superconductive carbon black, ZnOw, the conductive materials such as potassium titanate crystal whisker, resistivity that can the decrease polypropylene fibre; Can also improve the fracture strength of fiber, have good electric conductivity and durability, particularly under low humidity, still have good durablely from natural disposition electric conductivity, therefore in the field such as industrial, civilian very large purposes be arranged.
The specific embodiment
The present invention will be described in detail below in conjunction with specific embodiment: the manufacture method of conducting polypropylene fiber of the present invention, and this manufacture method adopts following steps:
A) getting 12-18 part characterization parameter diameter by mass fraction is 0.2-1um, and length is the four acicular type zinc oxide crystal whisker of 5-15um; 3-8 part characterization parameter diameter is 0.2-0.6um, and length is the electric conductivity potassium titanate crystal whisker of 5-12um; After above-mentioned material mixed, at 300-400 ℃ of vacuum kiln roasting 4-6h; With calgon dispersed with stirring in absolute ethyl alcohol, atmospheric plasma is processed 10-20min after the cooling; With 60-70 ℃ of loose, the cleaning 25-35min of deionized water for ultrasonic wavelength-division that contains calcium stearate dispersion, get solution upper strata suspension whisker and filter through 100 orders～150 orders, get the modified crystal whiskers mixed liquor, and repetitive operation 3-5 time is until filtering; In the vacuum drying oven oven dry, obtain the modified crystal whiskers mixture after the filtering;
B) get steps A by mass fraction) modified crystal whiskers mixture 6-10 part of obtaining, antimony doped tin oxide conducting powder 3-5 part, superconductive carbon black 7-17 part, aluminate coupling agent 0.2-0.4 part, Tissuemat E 1.7-3.0 part, PP-g-MAH bulking agent 1.2-2.5 part, mixer 250-400 turns/the airtight stirring reaction 45-60min of min under 60-70 ℃ of condition; And then adding isotactic polypropylene powder 100-120 part, 300-400 turns/min stirs 30-45min, obtains conducting electricity the isotactic polypropylene blend;
C) with step B) the conduction isotactic polypropylene blend that obtains at the dynamic vacuum oven drying to moisture content≤35ppm, directly extrude at the parallel dual-screw melting extruder that mixes, having the PP of compatibility or PE to make conduction isotactic polypropylene blend through composite spinning by core-skin mass ratio 20-30 ﹕ 80-70 and other is the polypropylene conductive fiber of cortex.
Embodiment of the present invention can carry out arbitrarily data replacement in above-mentioned disclosed data area, in order to consist of numerous embodiment, following examples only are cases, embodiments of the present invention are not made any restriction.
Embodiment 1:
The manufacture method of conducting polypropylene fiber of the present invention, this manufacture method adopts following steps:
Steps A) getting 15 parts of characterization parameter diameters by mass fraction in is 0.2-1um, and length is the four acicular type zinc oxide crystal whisker of 5-15um; 5 parts of characterization parameter diameters are 0.2-0.6um, and length is the electric conductivity potassium titanate crystal whisker of 5-12um; After above-mentioned material mixed, at 350 ℃ of vacuum kiln roasting 4-6h; With calgon dispersed with stirring in absolute ethyl alcohol, atmospheric plasma is processed 10-20min after the cooling; Then with 60-70 ℃ of loose, the cleaning 30min of deionized water for ultrasonic wavelength-division that contains calcium stearate dispersion, get solution upper strata suspension whisker and filter through 120 orders, get the modified crystal whiskers mixed liquor, and repetitive operation 3-5 time is until filtering; In the vacuum drying oven oven dry, obtain the modified crystal whiskers mixture after the filtering;
Step B) in, get steps A by mass fraction) 8 parts in the modified crystal whiskers mixture that obtains, 4 parts of antimony doped tin oxide conducting powder, 10 parts of superconductive carbon blacks, 0.3 part of aluminate coupling agent, 2.0 parts of Tissuemat Es, 2.0 parts of PP-g-MAH bulking agents, mixer 320 turns/the airtight stirring reaction 50min of min under 65 ℃ of conditions; And then add 100 parts in isotactic polypropylene powder, and 350 turn/min stirs 38min, obtain conducting electricity the isotactic polypropylene blend.
C) with step B) the conduction isotactic polypropylene blend that obtains at the dynamic vacuum oven drying to moisture content≤35ppm, directly extrude at the parallel dual-screw melting extruder that mixes, having the PP of compatibility or PE to make conduction isotactic polypropylene blend through composite spinning by core-skin mass ratio 25 ﹕ 75 with other is the polypropylene conductive fiber of cortex.
Embodiment 2:
The manufacture method of conducting polypropylene fiber of the present invention, this manufacture method adopts following steps:
A) getting 12 parts of characterization parameter diameters by mass fraction is 0.2-1um, and length is the four acicular type zinc oxide crystal whisker of 5-15um; 3 parts of characterization parameter diameters are 0.2-0.6um, and length is the electric conductivity potassium titanate crystal whisker of 5-12um; After above-mentioned material mixed, at 300 ℃ of vacuum kiln roasting 4h; With calgon dispersed with stirring in absolute ethyl alcohol, then atmospheric plasma is processed 10min after the cooling; Loose with 60 ℃ of deionized water for ultrasonic wavelength-divisions that contain calcium stearate dispersion, clean 25min, get solution upper strata suspension whisker and filter through 100 orders, get the modified crystal whiskers mixed liquor, and repetitive operation 3 times is until filtering; In the vacuum drying oven oven dry, obtain the modified crystal whiskers mixture after the filtering;
B) get steps A by mass fraction) 6 parts in the modified crystal whiskers mixture that obtains, 3 parts of antimony doped tin oxide conducting powder, 7 parts of superconductive carbon blacks, 0.2 part of aluminate coupling agent, 1.7 parts of Tissuemat Es, 1.2 parts of PP-g-MAH bulking agents, mixer 250 turns/the airtight stirring reaction 45min of min under 60 ℃ of conditions; And then add 100 parts in isotactic polypropylene powder, and 300 turn/min stirs 30min, obtain conducting electricity the isotactic polypropylene blend;
C) with step B) the conduction isotactic polypropylene blend that obtains at the dynamic vacuum oven drying to moisture content≤35ppm, directly extrude at the parallel dual-screw melting extruder that mixes, having the PP of compatibility or PE to make conduction isotactic polypropylene blend through composite spinning by core-skin mass ratio 20 ﹕ 80 with other is the polypropylene conductive fiber of cortex.
Embodiment 3:
The manufacture method of conducting polypropylene fiber of the present invention, this manufacture method adopts following steps:
A) getting 18 parts of characterization parameter diameters by mass fraction is 0.2-1um, and length is the four acicular type zinc oxide crystal whisker of 5-15um; 8 parts of characterization parameter diameters are 0.2-0.6um, and length is the electric conductivity potassium titanate crystal whisker of 5-12um; After above-mentioned material mixed, at 400 ℃ of vacuum kiln roasting 6h; With calgon dispersed with stirring in absolute ethyl alcohol, then atmospheric plasma is processed 20min after the cooling; Loose with 70 ℃ of deionized water for ultrasonic wavelength-divisions that contain calcium stearate dispersion, clean 35min, get solution upper strata suspension whisker and filter through 150 orders, get the modified crystal whiskers mixed liquor, and repetitive operation 5 times is until filtering; In the vacuum drying oven oven dry, obtain the modified crystal whiskers mixture after the filtering;
B) get steps A by mass fraction) 10 parts in the modified crystal whiskers mixture that obtains, 5 parts of antimony doped tin oxide conducting powder, 17 parts of superconductive carbon blacks, 0.4 part of aluminate coupling agent, 3.0 parts of Tissuemat Es, 2.5 parts of PP-g-MAH bulking agents, mixer 400 turns/the airtight stirring reaction 60min of min under 70 ℃ of conditions; And then add 120 parts in isotactic polypropylene powder, and 400 turn/min stirs 45min, obtain conducting electricity the isotactic polypropylene blend;
C) with step B) the conduction isotactic polypropylene blend that obtains at the dynamic vacuum oven drying to moisture content≤35ppm, directly extrude at the parallel dual-screw melting extruder that mixes, having the PP of compatibility or PE to make conduction isotactic polypropylene blend through composite spinning by core-skin mass ratio 30 ﹕ 70 with other is the polypropylene conductive fiber of cortex.
Claims (2)
1. the manufacture method of a conducting polypropylene fiber is characterized in that this manufacture method comprises the steps:
A) getting 12-18 part characterization parameter diameter by mass fraction is 0.2-1um, and length is the four acicular type zinc oxide crystal whisker of 5-15um; 3-8 part characterization parameter diameter is 0.2-0.6um, and length is the electric conductivity potassium titanate crystal whisker of 5-12um; After above-mentioned material mixed, at 300-400 ℃ of vacuum kiln roasting 4-6h; With calgon dispersed with stirring in absolute ethyl alcohol, then atmospheric plasma is processed 10-20min after the cooling; With 60-70 ℃ of loose, the cleaning 25-35min of deionized water for ultrasonic wavelength-division that contains calcium stearate dispersion, get solution upper strata suspension whisker and filter through 100 orders～150 orders, get the modified crystal whiskers mixed liquor, and repetitive operation 3-5 time is until filtering; In the vacuum drying oven oven dry, obtain the modified crystal whiskers mixture after the filtering;
B) get steps A by mass fraction) modified crystal whiskers mixture 6-10 part of obtaining, antimony doped tin oxide conducting powder 3-5 part, superconductive carbon black 7-17 part, aluminate coupling agent 0.2-0.4 part, Tissuemat E 1.7-3.0 part, PP-g-MAH bulking agent 1.2-2.5 part, mixer 250-400 turns/the airtight stirring reaction 45-60min of min under 60-70 ℃ of condition; And then adding isotactic polypropylene powder 100-120 part, 300-400 turns/min stirs 30-45min, obtains conducting electricity the isotactic polypropylene blend;
C) with step B) the conduction isotactic polypropylene blend that obtains at the dynamic vacuum oven drying to moisture content≤35ppm, directly extrude at the parallel dual-screw melting extruder that mixes, having the PP of compatibility or PE to make conduction isotactic polypropylene blend through composite spinning by core-skin mass ratio 20-30 ﹕ 80-70 and other is the polypropylene conductive fiber of cortex.
2. the manufacture method of conducting polypropylene fiber according to claim 1 is characterized in that described manufacture method, wherein:
Steps A) getting 15 parts of characterization parameter diameters by mass fraction in is 0.2-1um, and length is the four acicular type zinc oxide crystal whisker of 5-15um; 5 parts of characterization parameter diameters are 0.2-0.6um, and length is the electric conductivity potassium titanate crystal whisker of 5-12um; After above-mentioned material mixed, at 350 ℃ of vacuum kiln roasting 4-6h; With calgon dispersed with stirring in absolute ethyl alcohol, atmospheric plasma is processed 10-20min after the cooling; Then with 60-70 ℃ of loose, the cleaning 30min of deionized water for ultrasonic wavelength-division that contains calcium stearate dispersion, get solution upper strata suspension whisker and filter through 120 orders, get the modified crystal whiskers mixed liquor, and repetitive operation 3-5 time is until filtering; In the vacuum drying oven oven dry, obtain the modified crystal whiskers mixture after the filtering;
Step B) in, get steps A by mass fraction) 8 parts in the modified crystal whiskers mixture that obtains, 4 parts of antimony doped tin oxide conducting powder, 10 parts of superconductive carbon blacks, 0.3 part of aluminate coupling agent, 2.0 parts of Tissuemat Es, 2.0 parts of PP-g-MAH bulking agents, mixer 320 turns/the airtight stirring reaction 50min of min under 65 ℃ of conditions; And then add 100 parts in isotactic polypropylene powder, and 350 turn/min stirs 38min, obtain conducting electricity the isotactic polypropylene blend.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103173886A (en) * | 2013-04-08 | 2013-06-26 | 周焕民 | Method for manufacturing nylon conductive fibers |
| CN105734714A (en) * | 2016-02-23 | 2016-07-06 | 江苏华洋尼龙有限公司 | Polyethylene-polypropylene electroconductive composite fiber |
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| JPS63270860A (en) * | 1987-04-24 | 1988-11-08 | 東洋紡績株式会社 | Production of conductive composite fiber |
| CN1483863A (en) * | 2003-07-29 | 2004-03-24 | 东华大学 | Method for preparing whisker material to make modification treatment of spinning chemical fibre |
| CN101492839A (en) * | 2008-01-23 | 2009-07-29 | 周焕民 | Method for producing core-skin type inner conductive fiber |
| CN102409421A (en) * | 2011-12-20 | 2012-04-11 | 中原工学院 | Preparation method of carbon nanotubes/nano ATO (antimony tin oxide)/polypropylene electroconductive fibers |
-
2012
- 2012-11-26 CN CN201210491379.1A patent/CN102978738B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63270860A (en) * | 1987-04-24 | 1988-11-08 | 東洋紡績株式会社 | Production of conductive composite fiber |
| CN1483863A (en) * | 2003-07-29 | 2004-03-24 | 东华大学 | Method for preparing whisker material to make modification treatment of spinning chemical fibre |
| CN101492839A (en) * | 2008-01-23 | 2009-07-29 | 周焕民 | Method for producing core-skin type inner conductive fiber |
| CN102409421A (en) * | 2011-12-20 | 2012-04-11 | 中原工学院 | Preparation method of carbon nanotubes/nano ATO (antimony tin oxide)/polypropylene electroconductive fibers |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103173886A (en) * | 2013-04-08 | 2013-06-26 | 周焕民 | Method for manufacturing nylon conductive fibers |
| CN103173886B (en) * | 2013-04-08 | 2016-01-06 | 周焕民 | A kind of manufacture method of polyamide fibre conductive fiber |
| CN105734714A (en) * | 2016-02-23 | 2016-07-06 | 江苏华洋尼龙有限公司 | Polyethylene-polypropylene electroconductive composite fiber |
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